CN106784089A - A kind of preparation method of self-trapping smooth zno-based transparent conducting glass - Google Patents
A kind of preparation method of self-trapping smooth zno-based transparent conducting glass Download PDFInfo
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- CN106784089A CN106784089A CN201611188428.9A CN201611188428A CN106784089A CN 106784089 A CN106784089 A CN 106784089A CN 201611188428 A CN201611188428 A CN 201611188428A CN 106784089 A CN106784089 A CN 106784089A
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- 239000011521 glass Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000011324 bead Substances 0.000 claims abstract description 26
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 22
- 238000004544 sputter deposition Methods 0.000 claims abstract description 22
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 20
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 20
- 239000007791 liquid phase Substances 0.000 claims abstract description 8
- 238000012876 topography Methods 0.000 claims abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000002834 transmittance Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 30
- 238000004528 spin coating Methods 0.000 description 9
- 239000003595 mist Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 3
- 235000008216 herbs Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000005361 soda-lime glass Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 210000002268 wool Anatomy 0.000 description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Surface Treatment Of Glass (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
Abstract
The present invention discloses a kind of preparation method of self-trapping smooth zno-based transparent conducting glass, comprises the following steps：S1, using magnetron sputtering technique, the zno-based film under glass substrate surface sputtering growth；S2, using liquid phase method, prepare the SiO of the discrete distribution of individual layer in lower zno-based film surface2Bead template layer；S3, using magnetron sputtering technique, in SiO2The upper zno-based film of growth is sputtered on bead template layer, the thickness of upper zno-based film is less than SiO2The diameter of bead, obtains self-trapping smooth zno-based transparent conducting glass of the surface topography in concavo-convex textured structure；With reference to magnetron sputtering and the intrinsic advantages of liquid phase method plated film, in the preparation, SiO2Bead surface micro-structural can be adjusted as needed so that the surface micro-structure of upper zno-based film is easily controlled, and forms the surface micro-structure of excellent in uniform, realizes high transmittance, low resistance, preparation process is simple, reduces cost, beneficial to popularization and application.
Description
Technical field
The present invention relates to transparent conducting glass technical field, specifically a kind of system of self-trapping smooth zno-based transparent conducting glass
Preparation Method.
Background technology
Zno-based transparent conducting glass due to have concurrently the transparency and electric conductivity, and possess raw material be easy to get, it is environment-friendly, change
The advantages of learning good stability, therefore in many fields, such as photoelectron detector, photovoltaic device, film（Photoelectricity）Transistor, liquid crystal
The all existing important application prospect of the aspects such as display, sensor, heat reflector.
And self-trapping smooth zno-based photoelectric functional glass is a class high transmittance, low-resistivity and with fine surface micro-structural
Functional glass, be that a class is expected to obtain the novel inorganic nonmetallic materials of important application in terms of thin-film solar cells.
In the application of the window layer material of thin-film solar cells, due to possessing fine surface micro-structural, compared to biography
System zno-based photoelectric functional glass, self-trapping smooth zno-based photoelectric functional glass has transmitance and bigger mist degree higher, passes through
Increase the sunken light ability of Window layer, light path of the sunshine in Window layer can be extended, so that absorption of the device to sunshine is improved, it is right
Improve its light conversion efficiency and stability plays key effect.
When preparing self-trapping smooth ZnO transparent conducting glass at present, typically using following several method：
First, self making herbs into wool AZO of collosol and gel (sol-gel), environment is harsher for preparing needed for this method industrialization, and colloidal sol is steady
Qualitative contrlol is more difficult, and prepared membrane structure is loose；
2nd, chemical vapor deposition Direct precipitation matte TCO thin film, the method reaction condition control is complicated, and equipment cost is higher；
3rd, magnetron sputtering+acid wash making herbs into wool AZO, though the resistivity of the zno-based transparent conducting glass prepared by current magnetron sputtering
So can reach 5x10-4The order of magnitude of Ω cm, but because making herbs into wool is, by acid etching technique, to cause larger waste of material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of self-trapping smooth zno-based transparent conducting glass, prepared by the method
Process is simple, and it is uniform to obtain textured surface topography, surface micro-structure, and the controllable zno-based of surface topography is transparent leads
Electric glass, reduces production cost, it is easy to accomplish industrialization.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of self-trapping smooth zno-based transparent conducting glass, comprises the following steps：
S1, using magnetron sputtering technique, the zno-based film under glass substrate surface sputtering growth；
S2, using liquid phase method, prepare the SiO of the discrete distribution of individual layer in lower zno-based film surface2Bead template layer；
S3, using magnetron sputtering technique, in SiO2The upper zno-based film of growth, the thickness of upper zno-based film are sputtered on bead template layer
Degree is less than SiO2The diameter of bead, obtains self-trapping smooth zno-based transparent conducting glass of the surface topography in concavo-convex textured structure.
Further, the step S1 uses zno-based ceramic target, using Ar ions as sputter gas, dc source
With radio-frequency power supply collective effect in negative electrode, dc source sputtering power is 70W, and radio-frequency power supply sputtering power is 100~200W, target
Voltage is 110~210V, and the thickness for preparing lower zno-based film is 450~550nm.
Further, the step S2 prepares SiO2A diameter of 301~400nm of bead.
Further, the thickness that the step S3 prepares zno-based film is 200~300nm.
Further, glass substrate and the spacing of target are 70cm in the step S1 and S3.
The beneficial effects of the invention are as follows with reference to magnetron sputtering and the intrinsic advantages of liquid phase method plated film, using discrete distribution
SiO2Bead as micro-structural anti-reflection film system, the upper zno-based film above it with micro-structural anti-reflection film system as template, physical relief
Into concavo-convex textured structure；In the preparation, SiO2Bead surface micro-structural can be adjusted as needed so that upper zno-based
The surface micro-structure of film is easily controlled, and forms the surface micro-structure of excellent in uniform, realizes high transmittance, low resistance, prepares
Process is simple, reduces cost, beneficial to Industry Promotion application.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples：
Fig. 1 is schematic flow sheet of the invention；
Fig. 2 is the structural representation that the present invention prepares self-trapping smooth zno-based transparent conducting glass.
Specific embodiment
Embodiment one
With reference to shown in Fig. 1 and Fig. 2, the present invention provides a kind of preparation method of self-trapping smooth zno-based transparent conducting glass, including：
S1, using magnetron sputtering technique, the zno-based film 2 under the sputtering growth of the surface of glass substrate 1；
Specially：Soda-lime-silica glass with thickness as 1.1mm is glass substrate 1, and glass substrate 1 is placed in into magnetron sputtering chamber
It is interior, using zno-based ceramic target, the Ar gas of 30sccm is passed through as sputter gas, preparation temperature keeps room temperature；Zno-based ceramics
Target is preferably 70cm with the spacing of substrate；
During magnetron sputtering, using dc source and radio-frequency power supply collective effect in negative electrode, dc source sputtering power is 70W, is penetrated
Frequency power sputtering power is 100W, and target voltage is 210V, and operating pressure is 0.2Pa；Pre-sputtering first is carried out to glass substrate, is sputtered
Time 10min, then sputtering grows the lower zno-based film 2 that thickness is 500nm；
S2, using liquid phase method, prepare the SiO of the discrete distribution of individual layer on the lower surface of zno-based film 22Bead template layer 3；
Specially：Using spin coating device, with the SiO of percentage by weight 0.1%2Bead solution is spin coating liquid, rotating speed 2000r/
Min, spin coating 6 times, each 30s obtains SiO2Bead template layer 3, SiO2The small ball's diameter 301nm；
S3, using magnetron sputtering technique, in SiO2Sputter the upper zno-based film 4 of growth on bead template layer 3, technological parameter can be with
Step S1 is consistent, and the thickness of upper zno-based film 4 is 200nm, obtains self-trapping smooth ZnO of the surface topography in concavo-convex textured structure
Base transparent conducting glass.
Self-trapping smooth zno-based transparent conducting glass obtained above is carried out into mist degree test, transmission measurement, resistivity respectively
Test and XRD tests, mist degree is 13.2%, it is seen that light mean transmissivity is 84.9%, and resistivity is 9.6*10-4Ω cm, XRD
Spectrum shows that zno-based film stronger diffraction maximum, correspondence hexagonal wurtzite ZnO structures occurs in 2 θ=34.4 °（002）Diffraction maximum.
Embodiment two
With reference to shown in Fig. 1 and Fig. 2, the present invention provides a kind of preparation method of self-trapping smooth zno-based transparent conducting glass, including：
S1, using magnetron sputtering technique, the zno-based film 2 under the sputtering growth of the surface of glass substrate 1；
Specially：Soda-lime-silica glass with thickness as 1.1mm is glass substrate 1, and glass substrate 1 is placed in into magnetron sputtering chamber
It is interior, using zno-based ceramic target, the Ar gas of 30sccm is passed through as sputter gas, preparation temperature keeps room temperature；Zno-based ceramics
Target is preferably 70cm with the spacing of substrate；
During magnetron sputtering, using dc source and radio-frequency power supply collective effect in negative electrode, dc source sputtering power is 70W, is penetrated
Frequency power sputtering power is 150W, and target voltage is 130V, and operating pressure is 0.2Pa；Pre-sputtering first is carried out to glass substrate, is sputtered
Time 10min, then sputtering grows the lower zno-based film 2 that thickness is 450nm；
S2, using liquid phase method, prepare the SiO of the discrete distribution of individual layer on the lower surface of zno-based film 22Bead template layer 3；
Specially：Using spin coating device, with the SiO of percentage by weight 0.1%2Bead solution is spin coating liquid, rotating speed 2000r/
Min, spin coating 6 times, each 30s obtains SiO2Bead template layer 3, SiO2The small ball's diameter 400nm；
S3, using magnetron sputtering technique, in SiO2The upper zno-based film 4 of growth, upper zno-based film 4 are sputtered on bead template layer 3
Thickness be 300nm, obtain surface topography in concavo-convex textured structure self-trapping smooth zno-based transparent conducting glass.
Self-trapping smooth zno-based transparent conducting glass obtained above is carried out into mist degree test, transmission measurement, resistivity respectively
Test and XRD tests, mist degree is 15.8%, it is seen that light mean transmissivity is 83.2%, and resistivity is 7.4*10-4Ω cm, XRD
Spectrum shows that zno-based film stronger diffraction maximum, correspondence hexagonal wurtzite ZnO structures occurs in 2 θ=34.4 °（002）Diffraction maximum.
Embodiment three
With reference to shown in Fig. 1 and Fig. 2, the present invention provides a kind of preparation method of self-trapping smooth zno-based transparent conducting glass, including：
S1, using magnetron sputtering technique, the zno-based film 2 under the sputtering growth of the surface of glass substrate 1；
Specially：Soda-lime-silica glass with thickness as 1.1mm is glass substrate 1, and glass substrate 1 is placed in into magnetron sputtering chamber
It is interior, using zno-based ceramic target, the Ar gas of 30sccm is passed through as sputter gas, preparation temperature keeps room temperature；Zno-based ceramics
Target is preferably 70cm with the spacing of substrate；
During magnetron sputtering, using dc source and radio-frequency power supply collective effect in negative electrode, dc source sputtering power is 70W, is penetrated
Frequency power sputtering power is 200W, and target voltage is 110V, and operating pressure is 0.2Pa；Pre-sputtering first is carried out to glass substrate, is sputtered
Time 10min, then sputtering grows the lower zno-based film 2 that thickness is 550nm；
S2, using liquid phase method, prepare the SiO of the discrete distribution of individual layer on the lower surface of zno-based film 22Bead template layer 3；
Specially：Using spin coating device, with the SiO of percentage by weight 0.1%2Bead solution is spin coating liquid, rotating speed 2000r/
Min, spin coating 6 times, each 30s obtains SiO2Bead template layer 3, SiO2The small ball's diameter 350nm；
S3, using magnetron sputtering technique, in SiO2Sputter the upper zno-based film 4 of growth on bead template layer 3, technological parameter can be with
Step S1 is consistent, and the thickness of upper zno-based film 4 is 250nm, obtains self-trapping smooth ZnO of the surface topography in concavo-convex textured structure
Base transparent conducting glass.
Self-trapping smooth zno-based transparent conducting glass obtained above is carried out into mist degree test, transmission measurement, resistivity respectively
Test and XRD tests, mist degree is 17.1%, it is seen that light mean transmissivity is 82.8%, and resistivity is 6.1*10-4Ω cm, XRD
Spectrum shows that zno-based film stronger diffraction maximum, correspondence hexagonal wurtzite ZnO structures occurs in 2 θ=34.4 °（002）Diffraction maximum.
The above, is only presently preferred embodiments of the present invention, and any formal limitation is not made to the present invention；Appoint
What those of ordinary skill in the art, in the case where technical solution of the present invention ambit is not departed from, all using the side of the disclosure above
Method and technology contents make many possible variations and modification, or the equivalent reality for being revised as equivalent variations to technical solution of the present invention
Apply example.Therefore, every content without departing from technical solution of the present invention, is done according to technical spirit of the invention to above example
Any simple modification, equivalent, equivalence changes and modification, still fall within the range of technical solution of the present invention protection.
Claims (5)
1. a kind of preparation method of self-trapping smooth zno-based transparent conducting glass, it is characterised in that comprise the following steps：
S1, using magnetron sputtering technique, the zno-based film under glass substrate surface sputtering growth；
S2, using liquid phase method, prepare the SiO of the discrete distribution of individual layer in lower zno-based film surface2Bead template layer；
S3, using magnetron sputtering technique, in SiO2The upper zno-based film of growth, the thickness of upper zno-based film are sputtered on bead template layer
Degree is less than SiO2The diameter of bead, obtains self-trapping smooth zno-based transparent conducting glass of the surface topography in concavo-convex textured structure.
2. a kind of preparation method of self-trapping smooth zno-based transparent conducting glass according to claim 1, it is characterised in that institute
Step S1 is stated using zno-based ceramic target, using Ar ions as sputter gas, dc source and radio-frequency power supply collective effect in
Negative electrode, dc source sputtering power is 70W, and radio-frequency power supply sputtering power is 100~200W, and target voltage is 110~210V, is prepared
The thickness for obtaining lower zno-based film is 450~550nm.
3. a kind of preparation method of self-trapping smooth zno-based transparent conducting glass according to claim 1, it is characterised in that institute
State step S2 and prepare SiO2A diameter of 301~400nm of bead.
4. a kind of preparation method of self-trapping smooth zno-based transparent conducting glass according to claim 1, it is characterised in that institute
State step S3 prepare zno-based film thickness be 200~300nm.
5. a kind of preparation method of self-trapping smooth zno-based transparent conducting glass according to claim 1, it is characterised in that institute
The spacing for stating glass substrate and target in step S1 and S3 is 70cm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107579135A (en) * | 2017-09-06 | 2018-01-12 | 蚌埠玻璃工业设计研究院 | A kind of surface has the zno-based transparent conducting glass preparation method of micro-structural |
| CN107611188A (en) * | 2017-09-06 | 2018-01-19 | 蚌埠玻璃工业设计研究院 | A kind of multilayer film transparent conducting glass preparation method with micro-structural |
| CN107611187A (en) * | 2017-09-06 | 2018-01-19 | 蚌埠玻璃工业设计研究院 | A kind of matte multilayer film transparent conducting glass |
| CN109308952A (en) * | 2018-11-29 | 2019-02-05 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of flexible transparent conductive film of high low-resistance |
| CN109448922A (en) * | 2018-11-29 | 2019-03-08 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method of flexible electronic information glass |
| CN114394767A (en) * | 2021-12-27 | 2022-04-26 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method of red glass capable of reducing observation angle influence |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107579135A (en) * | 2017-09-06 | 2018-01-12 | 蚌埠玻璃工业设计研究院 | A kind of surface has the zno-based transparent conducting glass preparation method of micro-structural |
| CN107611188A (en) * | 2017-09-06 | 2018-01-19 | 蚌埠玻璃工业设计研究院 | A kind of multilayer film transparent conducting glass preparation method with micro-structural |
| CN107611187A (en) * | 2017-09-06 | 2018-01-19 | 蚌埠玻璃工业设计研究院 | A kind of matte multilayer film transparent conducting glass |
| CN109308952A (en) * | 2018-11-29 | 2019-02-05 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of flexible transparent conductive film of high low-resistance |
| CN109448922A (en) * | 2018-11-29 | 2019-03-08 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method of flexible electronic information glass |
| CN114394767A (en) * | 2021-12-27 | 2022-04-26 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method of red glass capable of reducing observation angle influence |
| CN114394767B (en) * | 2021-12-27 | 2023-08-22 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of red glass capable of reducing influence of observation angle |
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| CN106784089B (en) | 2018-05-01 |
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